CN114062443A - Flexible sensor for monitoring humidity of package headspace - Google Patents
Flexible sensor for monitoring humidity of package headspace Download PDFInfo
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- CN114062443A CN114062443A CN202111330098.3A CN202111330098A CN114062443A CN 114062443 A CN114062443 A CN 114062443A CN 202111330098 A CN202111330098 A CN 202111330098A CN 114062443 A CN114062443 A CN 114062443A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
Abstract
A flexible sensor for monitoring humidity of a package headspace relates to the field of humidity monitoring. Firstly, a flexible plastic film is used as a base material, an interdigital electrode substrate is printed by a screen printing process, and the electrode is covered by c-MWCNTs/GO/WS after being dried2Humidity-sensitive membranes formed of composite materials, wherein c-MWCNTs, GO, WS2The mass ratio of the three components is (1-4): (1-8): 1-4), and the mixture is put into a drying oven for drying to obtain the product based on c-MWCNTs/GO/WS2The flexible resistance type humidity sensor of (1). The sensor prepared by the method has a large humidity monitoring range, can quickly and accurately monitor the humidity change in the package, and has good repeatability.
Description
Technical Field
The invention relates to the field of humidity monitoring, in particular to a flexible sensor for monitoring humidity of a package headspace.
Technical Field
Intelligent packaging of food is an emerging technology that reduces waste, protecting consumer health and safety. Humidity is one of the most important factors influencing food quality, microorganisms grow rapidly when the humidity is too high, food is rotten rapidly, food water loss and quality reduction can cause problems of safety and resource waste when the humidity is too low, and the high rotting rate of the food and related diseases are fulminant due to improper humidity atmosphere. Traditional packing is mainly for the effect of playing protection, isolation, ration, decoration and explanation, but traditional packaging technology is owing to do not incorporate intelligent material, lacks monitoring, record and control to packing headspace humidity, consequently is necessary to install an intelligent humidity transducer and carries out real-time monitoring to packing inside humidity on fruit vegetables packing to in time take measures, regulation and control humidity range.
In recent years, two-dimensional layered transition metal chalcogenides (TMDCs), a low-cost, fast, directly printable 2D semiconductor material, have been used in the fields of gas, temperature, electronics, and opto-electronic sensing due to their excellent performance in nanoelectronics. The general formula of TMDCs is MX2Wherein M may be tin, tungsten, molybdenum, vanadium, etc., and X may be S, Se, Te, etc. Tungsten disulfide (WS)2) As one of the two-dimensional layered transition metal chalcogenides, the two-dimensional layered transition metal chalcogenide has a layered structure similar to graphene, has a large specific surface area and a tunable band gap, and shows great application potential in the aspect of humidity sensors.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a flexible humidity sensor capable of fast detection and a method for manufacturing the same.
The purpose of the invention is realized by the following technical scheme:
a flexible sensor for monitoring package headspace humidity is characterized by comprising an interdigital electrode printed on a flexible substrate film base material, and a filling sensitive layer c-MWCNTs/GO/WS coated on the interdigital electrode2。
Preferably, the flexible substrate is PET, PI.
Furthermore, the interdigital electrode is obtained by printing conductive silver paste or conductive carbon paste by a screen printing process, the number of interdigital pairs is 4-10, and the line width of the electrode is 0.1-0.5 mm.
The invention relates to a flexible sensor for monitoring package headspace humidity, namely, the sensor is based on c-MWCNTs/GO/WS2The preparation method of the flexible humidity sensor specifically comprises the following steps:
(1) printing interdigital electrodes on the surface of the flexible base material through a screen printing process, and drying to obtain a sensor base electrode layer;
(2) c-MWCNTs, GO and WS2Preparing a mixed solution according to the mass ratio of (1-4) - (1-8) - (1-4), pouring the mixed solution into a centrifugal tube, performing ultrasonic dispersion for not less than 2 hours, and coating the prepared humidity-sensitive mixed solution on the flexible electrode substrate prepared in the step (1).
Further, the drying temperature in the step (1) is 65 ℃, the time is 2 hours, and the uniform c-MWCNTs/GO/WS is formed by natural drying at room temperature after drying2And (3) a membrane.
Further, the length of the c-MWCNTs used in the step (2) is 0.5-2 μm.
Most of the conventional humidity sensors are based on rigid ceramics or Si/SiO2The substrate limits the application of the humidity sensor in some emerging industries, the flexible film is selected as the substrate, the prepared flexible humidity sensor has good flexibility, the cost is low, the process flow is simple and convenient, and the flexible humidity sensor can be applied in wider fields compared with the traditional rigid humidity sensor.
GO, an excellent nano-material, is composed of epoxy (-O), hydroxyl (-OH) and carboxyl (-COOH) groups covering the surface and edges. GO has proven to be an excellent sensing layer due to its humidity sensing ability, and its hydrophilicity is derived from its dangling bonds. However, when the humidity of pure GO is reduced, the time for removing water molecules is longer, so that the c-MWCNTs with hydrophobicity can be compounded, the time for removing and adsorbing water molecules can be shortened, and interaction force exists between the GO and delocalized electrons on a benzene ring of the c-MWCNTs due to pi-pi accumulation and electrostatic repulsion exists between GO molecules, so that the c-MWCNTs can be well dissolved in a GO solution. c-MWCNTs/GO/WS2The humidity sensor is exposed to a humid environment, and adsorbed water molecules are towards c-MWCNTs, GO and WS2Electrons are injected into the surface. Thus, n-type WS2The number of electrons in (1) increases and the concentration of holes in p-type GO decreases, resulting in further expansion of the depletion layer, followed by c-MWCNTs/GO/WS2The resistance of the humidity sensor changes.
Drawings
FIG. 1 shows a schematic diagram of a process of the present invention based on c-MWCNTs/GO/WS2Schematic electrode dimensions for the flexible humidity sensor of (1);
FIG. 2 is a schematic view of humidity sensor flexibility;
FIG. 3 is a response curve of the flexible humidity sensor in a humidity environment of 11-98% RH;
fig. 4 is a graph of the repeatability of a flexible humidity sensor switching back and forth between 11% and 98% RH in a humidity environment.
Detailed Description
Based on c-MWCNTs/GO/WS2Comprises a flexible substrate, an interdigital electrode and c-MWCNTs/GO/WS covered on the surface of the substrate2The composite material comprises c-MWCNTs with the length of 0.5-2 μm, GO and WS2The mass ratio is (1-4): (1-8): 1-4).
In order to better understand the invention, the invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to limit the invention in any way, i.e. the described examples are only a part of the examples of the invention, but not all examples.
Example 1: in this example, c-MWCNTs/GO/WS2The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking a certain mass of c-MWCNTs, dispersing the c-MWCNTs in a GO solution after 2h of ultrasound, and then taking a set mass of WS2Performing ultrasonic treatment for 2h again after mixing, and uniformly mixing for 30min by a vortex mixer to form c-MWCNTs/GO/WS2Composite solution of c-MWCNTs/GO/WS2The mass ratio of (A) to (B) is 4:2: 1.
Step 2) preparing an interdigital electrode: pretreating the flexible base material, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. Customizing 8 pairs of interdigital pairs and a silk screen plate with the electrode line width of 0.5mm, sequentially printing conductive silver paste on the base film by using a silk screen printer, putting the printed electrode into an oven, drying for 60min at 75 ℃, and naturally drying at room temperature for later use.
Step 3) pretreating the interdigital electrode prepared in the step 2), cleaning the surface of the electrode by using deionized water and absolute ethyl alcohol in sequence, fully drying the electrode in a nitrogen environment, and then carrying out a dropping coating method on the c-MWCNTs/GO/WS obtained in the step 1)2The composite solution is dripped on the surface of an interdigital electrode to form a composite gas-sensitive film, finally the electrode with the composite gas-sensitive film is placed into a drying oven to be dried at 65 ℃ for 2 hours, and is naturally dried at room temperature after being dried to prepare the c-MWCNTs/GO/WS2A humidity sensor.
The prepared flexible humidity sensor is placed in a humidity atmosphere of 11% RH, 23% RH, 33% RH, 43% RH, 59% RH, 75% RH, 85% RH and 98% RH obtained by a saturated salt solution method, a copper wire is led out to be in contact with a multimeter, and real-time resistance values of the sensor in different humidity environments are recorded by the multimeter connected with a computer.
FIG. 3 is a response curve of the flexible humidity sensor under different humidity, and it can be seen that the sensor has a good response in the humidity range of 11-98% RH.
Fig. 4 is resistance value data of the manufactured flexible humidity sensor in nine consecutive adsorption-desorption processes between the humidity of 11% RH and 98% RH, and it can be seen that the sensor has better stability and repeatability.
In this embodiment, the flexible substrate is PET.
Example 2: in this example, c-MWCNTs/GO/WS2The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking a certain mass of c-MWCNTs, dispersing the c-MWCNTs in a GO solution after 2h of ultrasound, and then taking a set mass of WS2Performing ultrasonic treatment for 2h again after mixing, and uniformly mixing for 30min by a vortex mixer to form c-MWCNTs/GO/WS2Composite solution of c-MWCNTs/GO/WS2The mass ratio of (A) to (B) is 2:1: 1.
Step 2) preparing an interdigital electrode: pretreating the flexible base material, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. Customizing 8 pairs of interdigital pairs and a silk screen plate with the electrode line width of 0.5mm, sequentially printing conductive carbon paste on a base film PI by using a silk screen printer, putting the printed electrode into an oven, drying for 60min at 75 ℃, and naturally drying at room temperature for later use.
Step 3) pretreating the interdigital electrode prepared in the step 2), washing the surface of the electrode by using deionized water and absolute ethyl alcohol in sequence, fully drying the electrode in a nitrogen environment, and then spraying the c-MWCNTs/GO/WS obtained in the step 1)2Spraying the composite solution on the surface of the interdigital electrode to form a composite gas-sensitive film, finally putting the electrode with the composite gas-sensitive film into a drying box for drying at 65 ℃ for 2 hours, and naturally drying at room temperature after drying to prepare the c-MWCNTs/GO/WS2A humidity sensor.
Example 3: in this example, c-MWCNTs/GO/WS2The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking a certain mass of c-MWCNTs, dispersing the c-MWCNTs in a GO solution after 2h of ultrasound, and then taking a set mass of WS2Performing ultrasonic treatment for 2h again after mixing, and uniformly mixing for 30min by a vortex mixer to form c-MWCNTs/GO/WS2Composite solution of c-MWCNTs/GO/WS2The mass ratio of (A) to (B) is 1:4: 1.
Step 2) preparing an interdigital electrode: pretreating the flexible base material, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. Customizing 10 pairs of interdigital pairs and a silk screen plate with the electrode line width of 0.2mm, sequentially printing conductive carbon paste on the base film PET by using a silk screen printer, putting the printed electrode into an oven, drying for 60min at 75 ℃, and naturally drying at room temperature for later use.
Step 3) pretreating the interdigital electrode prepared in the step 2), cleaning the surface of the electrode by using deionized water and absolute ethyl alcohol in sequence, fully drying the electrode in a nitrogen environment, and then carrying out a dropping coating method on the c-MWCNTs/GO/WS obtained in the step 1)2Coating the composite solution on the surface of the interdigital electrode to form a composite gas-sensitive film, finally putting the electrode with the composite gas-sensitive film into a drying oven for drying at 65 ℃ for 2 hours, and drying at room temperatureNaturally drying to prepare c-MWCNTs/GO/WS2A humidity sensor.
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (7)
1. A flexible sensor for monitoring package headspace humidity is characterized by comprising an interdigital electrode printed on a flexible substrate film base material, and a filling sensitive layer c-MWCNTs/GO/WS coated on the interdigital electrode2。
2. A flexible sensor for package headspace humidity monitoring according to claim 1, wherein said flexible substrate is PET, PI.
3. The flexible sensor for monitoring the humidity of the package headspace according to claim 1, wherein the interdigital electrode is obtained by printing conductive silver paste or conductive carbon paste by a screen printing process, the number of interdigital pairs is 4-10 pairs, and the line width of the electrode is 0.1-0.5 mm.
4. A method for preparing a flexible sensor for monitoring humidity of a package headspace according to any one of claims 1 to 3, comprising the following steps:
(1) printing interdigital electrodes on the surface of the flexible base material through a screen printing process, and drying to obtain a sensor base electrode layer;
(2) c-MWCNTs, GO and WS2Preparing a doping solution according to the mass ratio of (1-4) to (1-8) to (1-4), pouring the doping solution into a centrifugal tube, performing ultrasonic dispersion for not less than 2 hours, and then dropwise coating the prepared humidity-sensitive mixed solution on the flexible interdigital electrode substrate prepared in the step (1).
5. The method of claim 4, wherein the drying temperature in step (1) is 65 ℃ for 2h, and the dried product is naturally dried at room temperature to form uniform c-MWCNTs/GO/WS2And (3) a membrane.
6. The method according to claim 4, wherein the length of the c-MWCNTs used in the step (2) is 0.5 to 2 μm.
7. Use of a flexible sensor for package headspace humidity monitoring as claimed in any one of claims 1 to 3 for monitoring of food package headspace humidity.
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